A new route to synthesize new nanosized mixed ligand complexes of Zr(IV) have been investigated by the reaction of zirconium(IV) chloride with 3(2'-hydroxyphenyl)-5-(4-substituted phenyl)pyrazolines and ammonium salts of dithiophosphate, which after being treated with H 2 S gas acts as a precursor for ZrS 2. These complexes have been examined for crystalline/amorphous nature through XRD. The morphology of the complexes was studied by employing XRD which shows that all the complexes are amorphous solid. Molecular weight measurements, elemental analysis in conjugation with spectroscopic (IR, 1 H NMR, 31 P NMR) studies reveal dimeric nature of the complexes, in which dithiophosphate and pyrazoline are bidentate. Scanning electron microscopic images indicate that the particles are in a nano range. Putting all the facts together, coordination number six is proposed for zirconium with octahedral geometry.